Reducing-sugar product



I Patented Aug. 8, me

e. 1 i i a gm I e swam. mm I h an reducing 10 of makinz the same, inwhih'the dextrose equivnlenteontent oi the is relsfl'veiv hi h and thepmductj-is d a liquid than 61' Qhe aamidextmse equivalent analysis m1edncent'r'ation heretofore.

ll An n liditibnal object is the provision of nn improved conversionwherein a starch susp nsion is treated w'ith'an acid in the presence 'olto inhibit mtallizatibn of the rednbing sugar as nmm- 7 @1 Anotherbbiect is the nrodufibnbi a stlunh conversion product ia. -relaqtiv'elylow speciflc tqtatibn tor the ednteut thereof; i r

a! In efinversion er a. in a pension isti'eated with an aeidfiathascmor'ic acid at. ten

= to acid is ro prodfice amuse ,the mainversion is Chopped 5w thedextrose eqinvalmt content ot'the oemeraion #5 product has reached anextent where taste-imparting subetencee are produced. 'Ijhe remittingproduct is seam-less solution which ordinarily is concentratedto-mroximetely name. At this concentra'tidn fihere is tendency on the 40part of the new aiinf's contained in the eidenbie ammmt e'i when the:u-mm-tv gamma a): producing K II 1mm teem u m Afiri a u niecaqmwm'amewm chm an w m calla!- theinthe w 01m.aweifemmlsrintlznamflnonm13mmmeiiefatarmby Hamid as ordinarily Mead intheindmtrr. amml slowly and n n mayhem-melted may. I to dame I menu amind imam!!! to: soft crystillme mus, the-mas mayhemelfied m lent m'ndmdat comi has tween-flute! so mined! pal, m9

starch-hydrolyzed liquor of corresponding dextrose equivalent content.

In the lower dextrose equivalent range the relation between dextroseequivalent content and polarization in normally hydrolyzed starchliquors and liquors hydrolyzed in the presence of molybdenurn compoundsmay be close together. At a dextrose equivalent analysis of about 50arecognizable divergence appears and this divergence becomes pronouncedas the dextrose equivalent increases. A preferred product produced in accordance with the process described herein con-- sists of astarch-converted liquor within the dextrose equivalent range of 85 and90, the starch having been hydrolyzed by an acid in the presence of amolybdenum compound. This product will be a high dextrose equivalent,high fermentable syrup of slow crystallizing tendencyand of such limitedcrystallizing power that the final product sets into a soft fondant ormassecuite.

with a normal converted starch liquor the purity point at whichcrystallization .may be expected to occur to an obiectionable extentlies at about 66. This corresponds to a fermentable extract of about62.5 per cent. A syrup which will not crystallize may be produced inaccordance with my process having a dextrose equivalent analysis of '10and a fermentable extract of about 66. Thus, it is possible to produce afermentable liquor having a dextrose equivalent of substantially morethan 66 and a fermentable extract of substantially more than 62.5 percent which will not crystallize, by converting the starch suspensionfrom which the liquor is producedin the presence of a molybdenum,compound catalyst. For producing non-crystallizing syrups, it isdesirable to carry the conversion in the presence of molybdenum to anextent sulficient to provide a purity of between 68 and '12. Thisproduct may be concentrated, for example, to between 40 and Baum. Theamount of fermentable material in liquors produced in accordance with myprocess may be greater for the same dextrose equivalent content than inthe case Of liquors converted normally.

In effecting the conversion. the amount of molybdenum catalyst employedmay be of the order of 0.013 per cent of the starch converted, thepercentage stated being expressed as molybdenum. If substantially lowerquantities of the catalyst are employed the desired results cannot beobtained in a reasonable time. Substantially larger quantities becomeuneconomical. The catalyst may. be present in the form of sodiummolybdate or other molybdates or compounds of the metal. Molybdic acidand compounds of molybdenum with the halogens may be employed.

sodium molybdate was added thereto. Approximately 215 pounds of 28 percent muriatic acid was added. The slurry was first posted in an .openconverter for 20 minutes. It then was placed in a closed converter at 45pounds steam pressure for approximately 45 minutes, the time Percentageof solids per cent- 87.5 Dextrose equivalent do 89.5 Specific rotationdo 44.0 Percentage of sodium chloride -do .70 pH 4.9

This product may be shipped in tank cars without setting up as a solidmass which cannot be removed.

The density, dextrose equivalent, and specific rotation can be varied bychanging the time of conversion, the amount of molybdenum catalyst usedand the extent of the final evaporation.

By the process described it is possible to produce a syrup having adextrose equivalent content of 68 per cent to 92 per cent and a densityof the order of 42 Baum or higher without the formation of a rigid massof crystals. An ordinary syrup of this dextroseequivalent content andconcentration would set up as a solid crystalline mass. Thus, a productof intermediate dextrose equivalent content can be obtained which willnot crystallize at all and a product of high dextrose equivalent contentmay be obtained which will have a retarded crystallization tendency andwhich will set 'up as a workable mass rather than as a solid rigid bodyas is the case with products produced by ordinary hydrolysis.

The specific rotation of ordinarily converted dextrose solutions isquite definte and by determining the specific rotation of such asolution the dextrose equivalent content of the solution can beestimated with accuracy. Likewise, if the dextrose equivalent content ofa reducing sugar solution is known, the specific rotation can beestimated accurately. A liquor hydrolyzed in the presence ofa'molybdenum catalyst as described in the example given herein will havea lower specific rotation than ordinarily converted liquor and betweenthe dextrose equivalents of '10 and 88 this difference may be tabulatedas follows:

Ordinary conversion Mo conversion Dextrose Specific Dextrose Specificequivalent rotation equivalent rotation 83 59 88 45 85 B5 85 55 so so v07. s 75 75 75. 5 70 0s 70 s1. 5

The specific rotation of the liquor produced by hydrolysis in thepresence of a molybdenum catalyst isseen to be substantially less thanan ordinary dextrose specific rotation, indicating that l the reducingsugars formed'in the presence of the molybdenum catalyst are ofdifferent structural characteristics than ordinary dextrose. Thisindication-is further. substantiated by the reduced tendency towardcrystallization.

The amount of catalyst employed obviously may be varied with acorresponding variation in II 2. The process of producing a starchconversion product, which comprises subjecting a starch suspension toacid hydrolysis in the presence of a molybdenum compound, and carryingthe conversion to an extent suflicient to provide a dextrose equivalentof more than 66 per cent.

3. The process oi. producing a starch conversion product which comprisessubjecting a starch suspension to acid conversion in the presence of amolybdenum compound to produce a liquor havins a dextrose equivalentcontent of from 68 to 72 per cent, and concentrating the resultingproduct to produce a non-crystallizing liquid.

4. The process of producing a starch conversion product, which comprisessubjecting a suspension of starch to acid hydrolysis in the presence oia molybdenum compound to produce a liquor having a dextrose equivalentanalysis oi between 85 CERTIFICA'I'E' OF Patent No. 2,169,051.

and 90, terminating the hydrolysis, and concentrating the resultingliquor to produce a slowly crystallizing mass which will set up in aworkable non-rigid crystalline body at ordinary temperatures.

5. A starch conversion product, comprising a partially crystallized massof reducing sugars produced by acid hydrolyzation of a starch suspensionin the presence of a molybdenum compound.

said mass having a dextrose equivalent content of between 85 and 90 percent, and a specific rotation of substantially less than 56.5 per cent.

6. A starch conversion product, comprising a partially crystallized massof reducing sugars produced by acid hydroiyzation oi a starch suspensionin the presence of a molybdenum compound, said mass having a dextroseequivalent content or between 85 and 90 per cent, and a specificrotation of not more than substantially 55.

7. A starch conversion product, comprising a non-crystaliizing solutionoi reducing sugar produced by acid hydrolysis of a starch suspension inthe presence of a molybdenum compound, said product having a dextroseequivalent content of between 65 and '70 per cent, a fermentable extractcontent of more than 62.5 per cent, and a lower speciiic rotation thanthat of a liquor of equivalent dextrose equivalent content converted inthe absence of said molybdenum compound.

DAVID .P. LANGLOIS.

CORRECTION.

' AugdetB, 1939.

, DAVID P. LANGLOIS.

It is hereby certified that error appears in the printed specificationof the above numbered patent requiring correction as follows: Page 1,second column, line 1 for the word "such" read normal; and that the saidLetters Patent shouldbe read with this correction therein that the samemay conform to the record of the case in the Patent Office.

Signed and sealed this 10th day of October, A. n. 1939.

(deal) Henry Van Arsdale, Acting Commissioner oi Patents.

2. The process of producing a starch conversion product, which comprisessubjecting a starch suspension to acid hydrolysis in the presence of amolybdenum compound, and carrying the conversion to an extent suflicientto provide a dextrose equivalent of more than 66 per cent.

3. The process oi. producing a starch conversion product which comprisessubjecting a starch suspension to acid conversion in the presence of amolybdenum compound to produce a liquor havins a dextrose equivalentcontent of from 68 to 72 per cent, and concentrating the resultingproduct to produce a non-crystallizing liquid.

4. The process of producing a starch conversion product, which comprisessubjecting a suspension of starch to acid hydrolysis in the presence oia molybdenum compound to produce a liquor having a dextrose equivalentanalysis oi between 85 CERTIFICA'I'E' OF Patent No. 2,169,051.

and 90, terminating the hydrolysis, and concentrating the resultingliquor to produce a slowly crystallizing mass which will set up in aworkable non-rigid crystalline body at ordinary temperatures.

5. A starch conversion product, comprising a partially crystallized massof reducing sugars produced by acid hydrolyzation of a starch suspensionin the presence of a molybdenum compound.

said mass having a dextrose equivalent content of between 85 and 90 percent, and a specific rotation of substantially less than 56.5 per cent.

6. A starch conversion product, comprising a partially crystallized massof reducing sugars produced by acid hydroiyzation oi a starch suspensionin the presence of a molybdenum compound, said mass having a dextroseequivalent content or between 85 and 90 per cent, and a specificrotation of not more than substantially 55.

7. A starch conversion product, comprising a non-crystaliizing solutionoi reducing sugar produced by acid hydrolysis of a starch suspension inthe presence of a molybdenum compound, said product having a dextroseequivalent content of between 65 and '70 per cent, a fermentable extractcontent of more than 62.5 per cent, and a lower speciiic rotation thanthat of a liquor of equivalent dextrose equivalent content converted inthe absence of said molybdenum compound.

DAVID .P. LANGLOIS.

CORRECTION.

' AugdetB, 1939.

, DAVID P. LANGLOIS.

It is hereby certified that error appears in the printed specificationof the above numbered patent requiring correction as follows: Page 1,second column, line 1 for the word "such" read normal; and that the saidLetters Patent shouldbe read with this correction therein that the samemay conform to the record of the case in the Patent Office.

Signed and sealed this 10th day of October, A. n. 1939.

(deal) Henry Van Arsdale, Acting Commissioner oi Patents.

